Iraqi National Journal Of Chemistry

Effect of nitrating agent on the degree of nitration of cellulose as a nitrogen content for cellulose nitrate has been studied . Cellulose nitrate prepared by reacting triple nitrating a gent (( conc, HNO3 , fuming H2SO4 and H2O )) with ( -cellulose ) which prepared previously from bleached linter cotton, that had been treated mechanically and chemically in Iraq . This research demonstrated that the nitrogen content for cellulose nitrate increase with increasing HNO3 and with decreasing H2O in nitrating agent , also fuming H2SO4 has a main rule as a dehydrant through the reaction . Also research stated that all ranges of industrial cellulose nitrate can be prepared by using nitrating agent containing HNO3 in the range of (( 21.8% - 25.24% by wt )) .

This research is the electrical Conductivity study for each of trimetheprim, amoxicillin trihydrate and isoniazid in conductivity water at different temperatures (288.15-313.15) Kelvin By using lee-Wheaton equation for symmetrical electrolytes (1:1), The conductivity parameters have been calculated. The equivalent conductivity at infinite dilution (). The ion pair association constant (KA) and the mean distance values between ion (R) at the best value of standard deviation (). It is found that the values of () and (R) for each drug increase with increasing temperature, while the values of KA are inversely proportional with temperature. By comparing these values, They follow the sequence: o: amoxicillin trihydrate < trimetheprim < ioniazedKA : isoniazid < trimethoprim < amoxicillin trihydrateR : ionized > trimethoprim > amoxicillin trihydrateAn accurate method for determination of these drugs by using conductometric titration method with hydrochloric acid and sodium hydroxide have been found to be good and sensitive comparing with (the standard addition and potentiometric titration methods) from encyclopedia.

This work is concerned with the synthesis of _unsaturated carbonyl compounds namly chalcones (1-10), through condensation of 2,5_dihydroxy acetophenone with different homo and hetero aromatic aldehydes under basic medium. These chalcones are used as synthones in synthesizing the target flavanones (11-20), via cyclization reaction using sodium hydroxide or sulfuric acid in absolute ethanol

In this work mexiletine hydrochloride (MH) [1-(2,6-(dimethylphenoxy)-2-aminopropane hyrochloride] has been determined spectrophotometrically, using methyl orange (MO) and xylenol orange (XO). The method involved the addition of 1.5ml 0.1% (MO) or 1.2ml 0.05% (XO) reagents to a certain amount of MH, standard or samples, containing between (5-20 μgml-1) MH. The mixture is shaken for (30 sec.) and diluted to about 23ml in case of MO and to 8ml in case of XO in volumetric flasks using distilled water. The pH was adjusted by adding 1ml phthalate buffer pH 2.8 to the MO mixture and finally completed to 25ml, or with NaOH and HCl to pH 5.5 in case of XO and completed to 10ml. The colored ion-pair formed between MH and the reagents were transferred into separating funnels and extracted using 5.5ml CH2Cl2 and were shaken for 30 – 60s. After separation, the organic or aqueous layers were used for constructing calibration curves for spectrophotometric measurements of MH at 429nm and 438nm in cases of MO and XO respectively. The blanks were carried out in exactly the same way throughout the whole procedure. Molar absorptivity(ε L.mol-1.cm-1), detection limit, limit of linearity(µg.ml-1) and r2 were: 4.2x103, 0.32, 4 and 0.9961 for (MH-MO) and 2.3x103, 1.35, 5 and 0.9961 for (MH-XO) respectively. The method was used with reasonable accuracy and precision of(1.6-3.6 E%) and (±1-3.6 S.D%) respectively, for the determination of (MH) in synthetic samples of real blood, urine and capsules.

In this study , the efficiency of waste charcoal derived from walnut shell and peach Nuclei from synthetic wastewater(EWA) has been studied . Batch adsorption experiments were carried out as a function of pH , adsorbent mass, EWA concentration, contact time and temperature . The pH of each solution was not controlled , this is because the net interaction between the adsorbent and EWA could be disturbed by the buffer solution , therefore , the experiments were carried out in a pH 2 to 4 . These experiments were done under room temperature and showed that the optimum weight of charcoal derived from Walnut shell was 0.2gm , equilibrium time was 60min. , removal % (86.2) and Kd (86.2) , While optimum weight of charcoal derived from peach Nuclei was 0.05gm , equilibrium time was 120min. , removal % was( 34.5 ) and Kd( 138). Thermodynamic parameters such as ΔH , ΔG , ΔS , were calculated . The adsorption process on charcoal derived from peach Nuclei was endothermic, while exothermic on charcoal derived from Walnut shell, the results were analyzed by the Langmiur and Freundlich equation .

A simple , rapid and sensitive spectrophotometric method for the determination of trace amounts of dopamine hydrochloride in aqueous solution is described. The method is based on a reaction between dopamine hydrochloride with the mixture of Fe+3 and hexacynoferrate(III) ions to form an intense Prussian blue color complex thathas a maximum absorption at 710nm with a molar absorptivity of 2.138x104l.mole-1.cm-1 and a sandell sensitivity of 8.862x10-6µg.cm-2. Under optimum reaction conditions the absorbance of the Prussian blue color complex were found to increase linearly with increase in concentration of dopamine hydrochloride in the range (0.4-12ppm) with a relative standard deviation of 0.138-0.350% and a relative error of -1.983 to 2.9%. The proposed method was successfully applied for the determination of the selected drug in pharmaceutical preparations with very good recoveries of 98.02- 103.02%.

A new spectrophotometric method is described for the determination of Cu(II) in analytical sample . The proposed method based on the formation violet complex with 2-[(3-Chloro-4,6-disulfanamide phenyl ) azo] -4,5-diphenyl imidazole (Cdsai) as a new chromogenic reagent in nutral media that has a maximum absorption at λmax 588 nm . Linearity was observed from 0.25-6.00 µg.ml-1 with detection limit and 0.15µg.ml-1 . The effect of chemical, physical and analytical parameter is evaluated.

The present work consist of synthesis and characterization of three modified PVC polymers containing mercapto and hydrazino cinnoline-deravitives as pendent groups in the repeating units were synthesized in this work according to the following: 1:- Reaction of PVC with 4- hydrazine- 5- methoxy cinnoline in THF solvent afforded the following modified polymer (P1) 2:- Treatment of PVC with 4-mercapto 5- methoxy cinnoline in THF solvent furnishes the following modified polymer (P2) 3:- Reaction of PVC polymer with a mixture of equall amount of 4- hydrazino and 4-mercapto-5-methoxy cinnoline yields the following modified PVC polymer (P3) Structures of all these modified polymers have been confirmed by spectral (FT-IR and UV) analyses. The results indicated the presence of cinnoline-deravitives rings in the polymeric chain.

Transition state study have been carried out through computational methods to investigated photolysis of Raxil DS2 in aqueous solution by sun light . Quantum methods (semiemprical &Ab-initio included in packaged Hyper Chem 6.02 program) have been used to determine the chemical structures and physical properties of the pesticide molecule , intermediates ,and the all probable transition states structures involved in the first cleavage step reaction. Energetic properties and chemical reactivity was calculated for every chemical moieties that’s participated in the photolysis reaction through surface potential energy calculations . Initiation steps of photolysis have been studied theoretically for the main bonds in pesticide molecules through surface potential stability calculation . Several transition states are suggested for all probable main bounds that’s give-up the first cleavage step of photolysis ,they are examined by the calculations of surface potential energy, to estimate the heat of formation, energy barrier, and Zero point energy .calculations are carried out by study the structures of all suspected fragments that are produced from these transition states. Heat change for complete photolysis reaction has been estimated computationally to know heat formation for every chemical component participated in this reactions. In the present work ,it has been found that Raxil DS2 pesticide have very reactive chemical bonds ,since it undergoes photolysis through C10-C12 bond by real transition state with energy barrier equal to 31.175 kCal mol -1 ,that’s equal to energy light of wave length of 916.440 nm .The first initiation step of photolysis reaction is endoenergetic with given up Two free radicals at 35.426 kCal mol-1 . completely photolysis reactions of Raxil DS2 in aqueous media is exothermic reactions with -656.6945 kCal mol-1 . Fifty six mole of water molecules are needed to Transform the pesticide molecule into sixteen mole of carbonic acids , hydrochloric acid , nitric acid , and hydrogen gas.

Indium metal react with (C3H4N3S)2 (L1) or (C5H14N3S2)2(L2)in refluxing toluene to give the compounds [In(L1)3] and [In(L2)3] through an oxidative addition reaction. Trinuclear complexes of general formulas [In(L1)3(MCl2)2] and [In(L2)3(MCl2)2] were prepared by a direct reaction of MCl2.6H2O, (M=Co, Ni) or CuCl2.2H2O and ZnCl2.XH2O with the above indium compounds. The prepared compounds and complexes were characterized by IR and UV/Vis spectra, conductivity measurement, magnetic measurements , metal content were determined spectrophotometrically and their biological activity were also determined.The electronic spectra and magnetic measurements indicate that the Co and Ni complexes have square plan and octahedral geometry, while the Cu complexes show the presence of tetrahedral and octahedral geometry.

Complexes containing mixed ligands of cobalt (II) and nickel (II) have been synthesized by the reaction of cobalt chloride or nickel chloride with isopropylacetonethiosemicarbazone (LH) and substituted cresols (3–Methyl–2 nitrophenol (L1H) or 3–Methyl–2–aminophenol (L2H) or 2–Methyl–3–nitrophenol (L3H) or 3–Methyl–4–nitrophenol (L4H) in mole ratio 1:2:1 metal: isopropylacetonethiosemicarbazone: cresol, respectively and characterized phyico–chemically. They have been found to have the general formulas [M(LH)2(L¯H)]CL2 or[M(LH]2(L¯nH)Cl]Cl and K[M(L)2L¯] or M(L)2(L¯n)(H2O)] in neutral and basic medium, respectively where M = Co(II) or Ni(II); LH = isopropylacetonethiosemicarbazone; L¯H = L1H or L2H; Ln¯H= L3H or L4H; L¯= deprotonated L1H or L2H; Ln¯= deprotonated L3H or L4H, respectively. Furthermore, the complexes have been found to be biologically active as demonstrated by antibacterial screening against seven human pathogenic bacterial strains. It has been found that the complexes were more effective agent than the ligand.

Six metal complexes of Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) with new Schiff base p-(N,N-dimethyl amino benzaldehyde) acetopheneden thiosemicarbazone (ABATSC) have been synthesized and characterized by elemental analysis, magnetic susceptibility, molar conductance, in addition of IR and electronic spectra. The result show that the functional groups was (–C=S) and (-CH=N-). It has been found that (ABATSC) act as a natural bidentate ligand . The suggest geometry of the complexes appears to be octahedral and expected for non electrolyte.

The present work include the synthesis and characterization of spiro azetidin-2-one which achieved and expected to have some biological activity . the first step include the treatment of primary aromatic amine with primary aromatic aldehydes in boiling ethanol to give schiff bases which reacted in the second step with carboxylic acid ( 1,3-dithia-2-carboxylicacid )in the presence of triethylamine with phosphorusoxychloride in dry dichloromethane under nitrogen atmosphere at 0°C. To give spiroazetidin-2- one.The new synthesized compound were identified by melting points and UV,FT. IR, Mass, 1H NMR and 13C NMR spectrum

The aim of the present study was to investigate the effect of substituents on the phenyl ring of aniline which influence the amino pKb depending on their position and electron-donating or electron-withdrawing nature. Theoretical physical properties of these substituents have been calculated by (AM1) and (PM3) method. These physical properties are steric energy, dipole moment, nitrogen charge, bond length, heat of formation, ionization potential, LUMO and electronic energy. The pKb values have been correlated with the calculated parameters. Clearly showed that the ionization potential and bond length parameters are affected directly on the pKb values (R= 0.97).

The project is aimed at the synthesis of some Schiff bases derived from benzaldehyde and salicylaldehyde with some amino acids as glycine, DL-alanine ß-alanine, and L- methionine, with a new alternative method. The development includes the use of 10-2mole sodium hydroxide as a new catalyst, which is added to the classical method of Schiff bases synthesis. This method is applied successfuly to the synthesis of six imines from compounds mentioned .The structures of these Schiff bases are confirmed by using physical methods, namely, melting points or boiling point, UV and IR spectra. Finally a new suggested mechanism for the reaction mechanism is given, which is composed from three steps, on of them is slow, the other two are fast .

The synthesis of new Schiff Bases have been achieved by interesting of aldol condensation product of two carbonyl compounds, the products have been treated with thioethane in type of Michael reaction, to produce Michael product, which finally was treated with different aromatic amines to give the Schiff Bases. These compounds have been characterized by spectroscopic methods ( FTIR , HNMR , UV-Vis ) , TLC and melting points.

The type two Diabetes Mellitus patients (independent DM2) was used to investigate the level of C-reactive protein CRP & ceruloplasmin oxidase activity CP. The study aimed to compare the effects of altering the glycemic index or the amount of carbohydrate (serum glucose) with C-reactive protein and CP activity in patients compare with control group. As a marker of systemic inflammation, raised CRP concentrations are still within the normal range have been associated with an increased inflammation of Diabetes Mellitus DM.The our experimental data reveal that ceruloplasmin oxidase enzymatic activity is a serum non-specific factor acting during the early and late stages of DM.Also this study aimed to compare the effect of raising blood sugar with levels of CRP & CP in DM2 patients.The Glucose kit method & CRP latex were used in present study, CRP kit which is based on immunological reaction between CRP antisera bound to biologically inert latex particles and CRP in the test specimens of patients with DM (13Female, 17Male median age years, range=30-65)yr & in control subjects (7F,14M ,age range=30-45) yr.The results are classified according to visible agglutination to:1- A positive result / is indicated by the obvious agglutination pattern of the latex, in a clear solution.2- A negative result: is indicated by no change in the latex suspension on the test slide.Then the results of the precipitin test correlated with the quantitative data on CRP. Ceruloplasmin oxidase activity measured by using the modified Rice method & phenylene diamine – 2HCl as a substrate . This study has found that CRP concentrations in patients with DM increased very clearly than normal subjects, and established that CRP conc. in male was more than in female for patients specimens. An increase in serum ceruloplasmin (CP) oxidase activity has also been indicated in both sex, higher activity noted in female than male.Abbreviations :CRP:C-reactive protein, mg/dl: milligram per diacelitter,BS:blood suger, CP: ceruloplasm in, F: Female, M: Male.DM2: Type Two Diabetes Mellitus

Copper and zinc concentration were measured in 14 patients with malignant lymphoma and 18 with benign tumors,higher levels of copper (154.2 ±36.7), (20.2 ±4.2)in sera and tissues respectively in patients having lymphoma when compared with those of benign tumors .estimation of zinc metals showed no significant decrease in sera of lymphoma patients but higher concentration (34.45±11.73) in tissues of them when compared with respect of benign tumors .The storing effect on copper and zinc concentration in tissue samples which were stored in both storage solution (normal saline and formalin ) were also studied .It was found that the copper concentration levels could be measured in tissue which was stored in normal saline up to fife days in benign tissues and up to three days in malignant tissues , and up to four days in benign tissues and up to seven days in malignant tissues for zinc determination .Using formalin as a storage solution , copper could be measured in tissue which was stored in formalin up to fife days in benign tissues and up to eight days in malignant tissues , and up to fife days in benign tissues and up to seven days in malignant tissues for zinc determination.

Breast tumor patients generally have more oxidative stress than normal females. This was clear from non significant (P>0.05) decrease in RBCs GSSG-Red but there was significant decrease (P<0.05) in serum GSSG-Red activity. The study had found that free radicals in malignant breast tumors were higher than benign tumors, therefore the activity of GSSG- Red might be used as markers for prognosis of the disease through previouse studies and present study.